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By M. G. Zabetakis

This publication contains highlights of a 4-hour lecture and demonstration by the Bureau of Mines on the fire and explosion hazards of flammable liquids and solids, oxidizing materials, corrosive liquids, and compressed gases. The authors first presented this material as part of a 2-week course given to officers and enlisted men at the U.S. Coast Guard's Dangerous-Cargo Handling School, established at Fort Eustis, Va., in 1959. The Bureau was asked to present the lecture and demonstration because of the extensive experience of its researchers in handling certain harardous commodities.

Jan 1, 1961

By Ivan F. Avery

The design productive capacity of natural-gasoline and cycling plants in the United States on January 1, 1960, was 54.6 million gallons per day, according to the Bureau of Mines biennial survey. This represents an increase of 5.8 million gallons per day during the 2-year period since the last survey. The major increases occurred in Louisiana, Oklahoma, New Mexico and Texas. In Utah, natural gasoline capacity was reported for the first tine at 320 thousand gallons per day as of January 1, 1960. The total number of plants increased from 584 on January 1, 1958, to 596 on January 1, 1960. However, the operating plants decreased from 558 to 555 in the same period.

Jan 1, 1961

By E. G. King

Many of the rare-earth oxides are now commercially available in pure form and they have a variety of potential technical uses. Thermodynamic data for these oxides, however, are rather sparse. It is one of the functions of the Bureau of Mines to fill the need for this type of information. This report gives the results of low-temperature heat-capacity and high-temperature heat-content measurements by the Bureau of Mines of lanthanum sesquioxide. The entropy at 298.15° K. was evaluated and heat-content and entropy increments above 298.15° K. were obtained to 1,800° K. The results were combined with the known heat of formation at 298.15° K. to derive heats and free energies of formation at higher temperatures. Sufficient information is now available to permit reliable thermodynamic calculations involving lanthanum sesquioxide within the temperature range 298° to 2,000° K.

Jan 1, 1961

By Joseph Grumer

An instrumented spherical vessel has been used for many years to study laminar combustion waves. Concurrent measurements of flame speed and pressure-rise rates have led to evaluations of burning velocities, the pressure dependence of the burning velocity, and the expansion ratios of the gases passing through the combustion wave. For the most part, these studies have involved flames initially at atmospheric or subatmospheric pressure. The old spherical vessel used by the Bureau of Mines was not designed for use at elevated pressures. Moreover, being made of wrought iron, it was susceptible enough to corrosion to prohibit its use with many combustible mixtures that figure in industrial research. In mid-1956, under sponsorship of the Office of Naval Research, the Bureau undertook the development of a stainless steel spherical vessel capable of withstanding explosions of gaseous mixtures at initial pressures as high as 20 atm. and initial temperatures as high as 250° C. The design called for a double array (cross) of closely spaced small windows for observation of the flame as it traversed the vessel and a piezoelectric transducer to measure concurrently pressure-rise rates. Because no commercial contractor was willing to bid on the construction of such a vessel, it was built at the Bureau's Bruceton machine shop.7

Jan 1, 1961

By W. A. Cole

This report covers the preliminary phase of an investigation of clays, shales, and certain rocks in Wisconsin to determine the feasibility of processing lightweight aggregate in the State. The study was extended to include rotary-kiln testing of a limited number of shale samples, and to an appraisal of the Maquoketa shale resources in eastern Wisconsin. A total of 45 samples of clays, shales, and other argillaceous rocks of Wisconsin were tested. The lower Maquoketa shale is the only material found to date that offers possibilities as a source of material that can be processed in a rotary kiln for lightweight aggregate. Bedrock occurrences of the Maquoketa shale are found in the eastern and southwestern parts of the State. The populous southeastern region of Wisconsin presents a large potential marketing area for lightweight aggregate. For this reason special study was directed to the Maquoketa shale in the eastern district.

Jan 1, 1961

By Leonard Obert

Subsidence to surface occurs in a large proportion of underground mines. Preliminary to any indication of subsidence on the surface, there is usually a breaking up and sloughing of the cover into the mine opening which, in a period of time ranging from minutes to many years, progresses to the surface, This process is referred to as subsurface subsidence. In many mining operations, information regarding the process of subsurface subsidence is important, For example, if there are buildings or other improvements on the surface, or if the direction of the subsurface subsidence might threaten other underground workings--such as shafts--or if the subsidence might be progressing in a direction which would fall outside the anticipated subsidence limits, the problem could assume special significance.

Jan 1, 1961

By K. E. Tame

The Bureau of Mines is studying possible modifications in conventional uranium ore-processing steps to confine and permit controlled disposal of radioactive wastes. Surveys of Ra226 contamination of liquid wastes from uranium mills indicated that the Vanadium Corporation of America plant at Durango, Colo., had one of the more urgent problems. A possible procedure for minimizing the waste disposal problem was to reuse the waste solution in the mill--in effect, erasing the need for disposal of liquid waste. In examining this possibility, interlocked bench-scale leaching and solvent extraction tests simulating the Durango flowsheet were made. The simulated reuse of barren raffinate for leaching and washing was carried through three separate campaigns of 9, 12, and 35 cycles each.

Jan 1, 1961

By John E. Shelton

The growing interest in beryllium as a structural material, and its in-creased use in recent years for atomic energy application, have led both government and industry to express concern over the inadequacy of the beryllium resources in the United States and the free world. Contemplated and proposed uses for this unique material will surpass the capacity of the domestic beryllium mining industry to supply raw material, which is presently extracted from relatively small deposits by hand sorting. The need for a simple beneficiation process for beryl ores has long been recognized by the Bureau of Mines, but to date no single process has proved satisfactory for treating deposits containing a sufficient tonnage of beryl ore to warrant commercial exploitation. As a part of the Bureau's continuing effort to develop an economical recovery process, this report describes flotation research on samples of beryl-bearing pegmatites from the George Roebling mine in Connecticut, and the Colony mine in New Hampshire. The study resulted in two methods of treatment to which the ores responded reasonably well.

Jan 1, 1961

By S. J. Gasior

Pilot plant studies showed the technical feasibility of fluidized-bed operation for producing hydrogen and synthesis gas by the steam-iron process. A mixture of iron and iron oxide from 20-to 100-mesh was partially reduced with a simulated producer gas and then oxidized with steam and/or carbon dioxide. Results of tests show the effects of pressure, temperature, bed height, gas-to-solids ratio, type of iron oxide, and composition of gas on the gas and solids conversions during reduction and oxidation. A baffled free-fall solids system was also found operable. The short residence time of about 5 seconds limited conversion of the solids.

Jan 1, 1961

By J. G. Croeni

The high thermal-neutron cross section of gadolinium and the good mechanical and corrosion properties of titanium suggest that alloys of these two metals might be useful as control rod material. To aid in establishing the feasibility of this combination, the Federal Bureau of Mines investigated the titanium-gadolinium system. The results indicate that the system is composed of a single eutectic reaction and a peritectoid reaction involving the alpha-beta transformation of titanium. The eutectic isotherm extends from 1 to 99 pct, gadolinium at 1,240° C. The established eutectic composition is about 95 pct, gadolinium. The peritectoid reaction occurs at 885° C. and extends almost over the entire composition range. Hardness increases slightly with additions of gadolinium, and little change is obtained by heat treatment. Alloys containing less than 10 pct. gadolinium are amenable to extensive cold-working, but alloys having higher percentage of gadolinium content are only moderately cold-workable. All alloys can be hot-worked in iron sheathing at 750° C. Observation indicates that all compositions possess good machinability. Corrosion resistance to water at room temperature is apparently poor, especially in the gadolinium-rich alloys. INTRODUCTION A combination of the good mechanical and corrosion properties of titanium and the variety of thermal-neutron cross sections characteristic of the rare-earth metals suggests that alloys of these metals may be used for control rod materials. For this reason the Bureau of Mines proposed a study of the titanium-gadolinium alloy system, and the Atomic Energy Commission sponsored the investigation.

Jan 1, 1961

By S. L. May

Procedures for separating columbium and tantalum have been developed by the Bureau of Mines as part of a broad research program on the utilization of low-grade ores of columbium and tantalum, Columbium and tantalum compounds of greater than 99 percent purity have been obtained by application of the solvent extraction separation system: Hydrofluoric acid-sulfuric acid-methyl iso-butyl ketone. This system is unique in that it not only separates columbium from tantalum, but also separates these two metals from other metallic impurities. The system is effective for separating the metals irrespective of the tantalum and columbium ratio of the starting materials. Investigations in which the spent feed obtained from the initial coextraction step was recycled to the system indicated that efficiency was increased, and cost was reduced without impairing product purity. Continuous tests demonstrated that this solvent extraction system could be used in large-scale equipment without loss in efficiency or in purity of products. The separation of columbium and tantalum has been difficult because of the similarity in their chemical bahavior. Many methods have been proposed for separating these two elements, but most methods either did not achieve satisfactory separation or were tedious and time consuming. The Marignac process (3, 4)4 developed in 1866 was the only method used commercially until recently. This separation procedure is based on the difference in solubility in aqueous solution of potassium tantalum fluoride and potassium columbium oxyfluoride. Current commercial practice appears to favor solvent extraction as a method for separating tantalum from columbium (1). Several efficient methods for separating columbium from tantalum by solvent extraction (2, 9, 8) were reported earlier from this laboratory.

Jan 1, 1961

By P. C. Good

The work reported here was undertaken by the Federal Bureau of Mines to investigate new methods of preparing high-purity metal. Tungsten hexachloride was prepared by direct chlorination of scrap tungsten metal and by treating tungstic oxide with carbon and chlorine. The resulting tungsten hexachloride was purified by distillation and reduced win: sodium, magnesium, or hydrogen. The metal prepared by these techniques was at very high purity after arc melting but of variable quality prior to arc meIting. Metal recovery ranged from about 40 to 90 percent of theoretical values, It was found possible to deposit a smooth, dense coating of high-purity tungsten on the inside of a heated tube by vapor-phase reduction of tungsten hexachloride at reduced pressure.

Jan 1, 1961

By C. F. Ellis

Interest in the composition of automobile exhaust gases has been greatly accelerated by recent studies that have indicated that these gases contribute to smog formation in urban areas. Several analytical methods have been published for the analysis of the hydrocarbons in the exhaust gases, but similar information has not been published on the analysis of the oxygenated compounds. This report presents procedures for chemical analyses of certain oxygenated compounds, procedures for sampling the exhaust gases for these analyses, and the analytical results of some experimental work in which these procedures were used. A stationary 1956 model, 170 horsepower, V-8, dynamometer-mounted engine, operated to simulate vehicular cruise conditions, was used for the study. Exhaust gases produced from a regular-grade Midcontinent gasoline during 15-40- , and 60-mile-per-hour cruise operations were analyzed by chemical methods for formaldehyde, total aldehydes, total carbonyls, total alcohols, carbon associated with the oxygenated compounds, and the oxides of nitrogen. Experimental results indicate: 1. The range of concentrations of the total of the functional groups of oxygenated compounds, expressed as moles per million moles of water-free exhaust gases, is about 90-100; the concentrations increase with engine speed. 2. Aldehydes comprise about 80-90 mole- percent of the total of the oxygenated groups, and formaldehyde accounts for about 50 mole-percent of the total aldehydes. 3. The order of magnitude of the concentration of the carbonyls is the same as that for the aldehydes, indicating that ketones are not a major group. A colorimetric test indicates that methyl ketones Constitute about 2 mole-percent of the oxygenated compounds.

Jan 1, 1961

By W. Dan Walker

In an effort to keep mine hoist accidents to a minimum and to impart to managers and workers the essential elements that enter into safe installation and maintenance of hoisting equipment, the Bureau of Mines presents this Information Circular as a guide. Hoisting of men and materials is an essential operation in many mines and has become so commonplace that some persons are likely to ignore day-to-day inspections or become lax in the operating phases. With proper maintenance and operation, hoists can be exceptionally safe. However, lack of strict attention can invite tragedy or costly shutdowns.

Jan 1, 1961

By William J. Campbell

The purpose of this investigation by the Federal Bureau of Mines was to design and construct a fluorescent X-ray spectrograph for dynamic rate studies of selective oxidation in molten metals and to establish basic principles for interpretation of data obtained by this method. An X-ray spectrograph was constructed in which the sample holder is a resistance wound furnace; it was operated up to 800° C. in oxidizing atmospheres. No difficulties were experienced with the cooling or heating systems nor with the protective layer of mica around the X-ray tube window, even though the oxidizing surface of the metal is only 0.5 inch from the X-ray tube window, Means are provided for heating under controlled atmospheres for selected time? temperature cycles.

Jan 1, 1961

By R. L. Marovelli

ANTICIPATING the eventual use of the huge tonnages of nonmagnetic taconites of the Mesabi range of the United States, the Federal Bureau of Mines is classifying and evaluating these deposits in detail. This introductory report describes work begun in 1954 as part of a long-range program to sample, classify, and evaluate important occurrences of nonmagnetic taconite on the Mesabi, range. Included in this report are brief discussions of the geology, history, and potential of the Mesabi range district and mining industry, together with a more detailed presentation of the sampling and metallurgical evaluation of these nonmagnetic taconite deposits. A total of 898 field samples was collected. Most of these were taken in the region between Grand Rapids and Chisholm, Minn., but a few came from the area between Chisholm and Buhl, Minn. Of the total samples, 865 were from open pit bank faces where the greater vertical distances presented by the cherty members facilitated the taking of a large number of samples. Conversely, the narrow face presented by the slaty members confined and limited the areas from which samples were taken. In addition, 33 of the field samples were taken from rock dumps in order to determine, in a preliminary way, the characteristics of these materials.

Jan 1, 1961

By R. P. Jewett

The object of this investigation was to correlate the crushing strength of green pellets prepared from magnetite, specular and earthy hematite with the particle size of these respective raw materials. In this study no attempt was made to correlate the strength of fired pellets and particle size. The effect of particle size upon a number of fine ores and concentrates was studied. Much of the low-grade ore reserves in the Lake Superior Region must be finely ground before concentration and then agglomerated for iron and steelmaking processes. Fine natural ores also must be agglomerated. Pellets constitute an important type of agglomerate. Considerable handling occurs during screening to remove undersize and oversize pellets, and in transfering green unfired pellets from the balling machines to the heat-hardening equipment. As a result the strength of the green pellets is a factor of great importance.

Jan 1, 1961

By K. K. Kershner

Nickel having a purity of more than 99.99 percent with reference to metallic impurities was electrodeposited at the Rolla Metallurgy Research Center of the Federal Bureau of Mines. The production of high-purity nickel is in keeping with the current trend in technologies for producing metals with lower and lower percentages of impurities. To understand more fully the role to be played by nickel by itself and as a component in many alloys, the element must be in a state of high purity. Procedures are outlined for purifying nickel solutions by precipitating and filtering off impurities. Details are given for using the purified solutions as electrolytes in depositing high-purity nickel. The elecneleposited nickel contained 0.0005 to 0.002 percent each of cobalt, copper, aid iron together with spectrographically detectable traces of aluminum, magnesium, and silicon. The deposits were smooth and dense; the crystalline structure was typical of an electrodeposited metal. Some preliminary experiments for purifying nickel solutions by liquid-liquid extraction are also described in this report. Tests of this type were limited since more encouraging results were obtained by other methods of purification.

Jan 1, 1961

By F. W. Wood

A program of research was conducted by the Bureau of Mines to investigate anomalies in electrical-discharge behavior during consumable-electrode arc melting of titanium and to study the effects of these irregularities on arc-furnace explosions. A major effort was devoted to an experimental survey of arc behavior and a qualitative definition of discharge phenomena.3/ An important conclusion was that the "glow" of industrial arc-melting terminology is not a glow discharge but a skittering arc in a displaced position. The conditions that permit displaced skittering were tentatively defined. The displaced skittering arcs tended to damage melting crucibles in two ways, and details of possible mechanisms leading to crucible rupture and explosive reactions have been proposed accordingly. However, no acceptable means of preventing crucible damage was discovered.

Jan 1, 1961

By D. Z. Hobbs

Because an economic method for preparing pure boron has not been developed, a program was started by the Bureau of Mines to evaluate existing techniques or to develop new methods for preparing the pure element. This report describes investigations directed toward the development of techniques for the preparation of pure boron by fused-salt electrolysis. Only two of the several fused-salt baths tested were satisfactory for the preparation of boron. These baths contained (1) potassium fluoride, lithium fluoride, potassium fluoborate and boron trioxide; and (2) potassium fluoride, potassium chloride, and boron trioxide. Of these two mixtures, the latter was more satisfactory. Elemental boron of from 90- to 95-percent purity and, in isolated cases, as high as 98-percent purity, was prepared from these two types of fused-salt baths. There appeared to be no distinct differences either in the yields or the purity of boron prepared at current densities ranging from 795 to 1,000 amperes per square foot. Current efficiencies were as high as 85 percent.

Jan 1, 1961